Scope of the Lecture

1. Development of Metrology of Chemical Measurements in EstoniaIvo LeitoUniversity of TartuEstonialeito@ut.ee

2. Scope of the Lecture • Metrology system in General • Present • Future • Metrology in Chemistry • A Recent Survey • Situation at Field Labs • Accreditation • Teaching/Training • International Collaboration

3. Metrology council Central Office of Metrology (Metrosert Ltd) The Metrology System in Estonia: the Current Structure MoEAC The NMI • National standards: • Mass, Length • Other: • Pressure, Force, Density • Temperature • Electrical quantities • Flow • etc.

4. Planning the Future • PHARE Projects: • ES 9903.01 National Metrology and Accreditation Centre • Aim: Strategy planning • ES 0102.01 Development of Conformity Assessment Infrastructure in the field of metrology • Aim: Investments

5. Strategy Planning Project • Donor: PHARE • Foreign experts: NMi VSL (Netherlands) • Estonian contractor: Ministry of Economic Affairs (MoEA) • Start: Jan 2002 • End: Dec 2002 • Initially metrology in chemistry was not included at all!

6. Strategy Planning Project • Extensive visits of Dutch experts • Two questionnaires targeted specifically to the needs and expectations of laboratories, incl industrial • Workshop at MoEA involving as many stakeholders as possible • Survey: Chemical Analyses and Measurements: the Needs of Estonia

7. The Main Problems Identified • In several fields no traceable calibration possibility is available • Status of the NMI is somewhat unclear • Poor International visibility. No membership in: • Metre convention, CIPM MRA • EUROMET, Eurachem • Low financing of metrology: • In Estonia 0.0004% of the GDP • Average in EU 0.005% of the GDP • Chemistry is split between ministries

8. Metrology council Technical University of Tallinn Central Office of Metrology (Metrosert Ltd) University of Tartu The Metrology System in Estonia: Planned Structure MoEAC The NMI • MiC • Chromatography-mass-spectrometry • pH metry • Spectrophotometry • Air Humidity • Air Flow Velocity • National standards: • Mass, Length, Temperature • Other: • Pressure, Force, Density • Electrical quantities • Time • Luminous intensity • etc. • MiC • Atomic Spectroscopy • Ion Chromatography • Surface Hardness • Surface Roughness

9. Spearheads • Distributed metrology system: • Metrosert Ltd + UT + TTU = NMI • Metrology system tuned to the needs of the country • CIPM MRA: • membership • registration of CMC-s • International and regional co-operation • EUROMET, Eurachem • Baltic collaboration

10. Investments Project • Donor: PHARE • Foreign experts: MIKES (Finland) • Estonian contractor: Ministry of Economic Affairs (MoEA) • Start: May 2003 • Planned End: Dec 2004 • Investments: 2 MEUR • equipment for chemistry: 0.5 MEUR

11. Functions of the MiC Centres at Universities • Providing traceability to field labs • Developing, maintaining and disseminating competence in MiC • Organising/mediating interlaboratory comparison measurements • Applied research tuned to the needs of the country • Supporting Governmental institutions • Supporting Accreditation

12. Survey: Chemical Measure-ments, the Needs of Estonia • There is ample general information that chemical measurements are highly important in Estonia • There is a lack of specific information • about the present volumes of chemical measurements • about the present and future needs in terms of types and volumes of chemical measurements • A Survey was conducted in 2002

13. Survey: Results The full report (in English) is available at: http://www.ut.ee/katsekoda/Chem_Needs

14. Survey: Results, Industry • Selected sectors: Food, Chemical, Water • The annual number of chemical measurements in the selected sectors of industry: • performed by the enterprises: 1.5 ± 0.3 M • ordered from Estonian laboratories: 0.025 ± 0.01 M • ordered from outside of Estonia: 500 ± 300

15. Survey: Results • The estimated annual volume of chemical measurements: • the whole Estonian industry: 1.9 ± 0.6 M • dedicated laboratories: 4.9 ± 1.0 M • the medical sector: 5.7 ± 2.0 M

16. Survey: Results The estimated total annual volume of chemical measurements in Estonia is 12.5 ± 2.3 millions

17. Survey Results: Trends

18. Survey Results: Types of Chemical Measurements

19. Survey: Results • Strong need for: • more different ILCs • more different CRMs • more training • only 6% of the industry and 0% of the dedicated laboratories’ respondents indicated that the competence is sufficient • a competence centre in chemical analysis

20. Survey: Results • Fields of chemical measurements that are currently uncovered were identified: • Contaminants: some pesticides, veterinary drugs, dioxins, ... • Food quality: selenium, dietary fibre, iodine, ...

21. MiC at Field Laboratories • Metrological principles form the basis of every measurement • Validated measurement procedures • Measurement uncertainty • Traceability • Independent assessment of performance • Their application is the responsibility of every laboratory

22. MiC at Field Laboratories • Validation is in general well established • Measurement uncertainty • most laboratories do at least something • the quality is often insufficient • Traceability • in many cases remains a mystery • most of the labs use CRM-s • price and availability are often obstacles

23. Interlaboratory Comparisons • Organised in Estonia: • Surface water • Ground water • Wastewater • From abroad: FAPAS/FEPAS, Aquacheck, etc. • IMEP • There is quite a wide range of measurements for which no ILCs are available

24. MiC is Important! Accreditation of Field Laboratories • Accreditation is required by a number of legislative acts (around 50) • 115 testing laboratories are accredited (01.01.03) • Out of them ca 50% perform chemical measurements Source: http://www.eak.ee/

25. Accreditation of Field Laboratories • Estonian Accreditation Centre has applied for the membership of the EA MLA • Preliminary assessment: March 2002 • Full assessment: March 2003 • Report on dealing with non-conformities: June 2003 • Possible acceptance to EA MLA: October 2003

26. Teaching and Training • University level teaching of chemistry: • University of Tartu (UT) • Tallinn Technical University (TTU)

27. Teaching and Training • Teaching MiC • Teaching of MiC at UT started in 1999 • MiC is now well established in the curricula of chemistry and materials science students • The course at present is voluntary, with the commencement of the 3+2 scheme it becomes obligatory • Teaching of MiC is also carried out at TTU

28. Teaching MiC • There is a dilemma: • On one hand: • It is desirable to make it clear for the students from the very beginning that Metrological aspects, and MU in particular, are an integral part of any measurement, not just a fancy add-on. • On the other hand: • Explaining the topics of MiC in full rigor before starting with analytical chemistry has low efficiency, because the concepts of MiC do not link to anything in the student's knowledge and will therefore be only partially understood and forgotten very quickly.

29. Teaching MiC at UT: 2 Stages • The First stage • The basics of MiC have now been introduced into the general analytical chemistry curriculum • Students get: • the very basis in lectures (measurement, measurement results, their comparability and traceability, measurement uncertainty, the ISO method of uncertainty estimation…) • practical training in laboratory classes: estimation of measurement uncertainty of real analyses performed by the students http://tera.chem.ut.ee/~ivo/akpr1/ http://tera.chem.ut.ee/~ivo/praks/

30. Teaching MiC at UT: 2 Stages • The second stage: Special Course on MiC • In addition to the basics in the general analytical chemistry curriculum there is a dedicated course on MiC • Topics covered: • Metrology, measurement, measurement unit, the SI system, measurement result, measurement uncertainty, comparability and traceability of measurement results, error and uncertainty, estimation of measurement uncertainty, the ISO procedure of uncertainty estimation, other procedures, possible uncertainty sources, uncertainty components, quantifying uncertainty components, metrology in chemistry, method validation, primary methods (gravimetry, titrimetry, coulometry, isotope-dilution mass-spectrometry), reference materials, certified reference materials, interlaboratory comparisons (ILCs), types of ILCs, proficiency testing schemes (PTSs), data treatment of results of PTSs, metrology system in Estonia, the metrology act, metrology in Europe and the World, standards, ISO standards, quality, quality management, quality systems, ISO 17025, accreditation, accreditation in Estonia

31. Teaching MiC at UT • The “Current Status” of teaching MiC at UT has been published: Accreditation and Quality Assurance (2002) 7:159-162 http://tera.chem.ut.ee/~ivo/metro/

32. Teaching MiC: Joint Activities of the Universities • There is a preliminary agreement to join forces between UT and TTU • Student Teaching Material on MiC will be published jointly

33. Training • University of Tartu offers training to laboratories • MiC • Experimental techniques (GC, HPLC, …), incl their MiC aspects • Practical aspects of work in laboratory • Efficient use of computers in laboratories • Education is if not the most important then at least one of the most important things in this field

34. International Collaboration • Still limited, but getting better • EUROMET • EC-JRC IRMM • The Baltic Countries. Plans: • joint projects and events • joint ILC-s • joint database of laboratories